#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:05:44 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180168 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/64/7106416.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7106416
loop_
_publ_author_name
'Eleni Kotsapa'
'Mark T. Weller'
_publ_section_title
;
 Vanadium fluoroarsenates-folding sheets into highly corrugated layers and
 crystalline arrays of large inorganic tubes
;
_journal_issue                   21
_journal_name_full               Chem.Commun.
_journal_page_first              6132
_journal_page_last               6134
_journal_paper_doi               10.1039/c1cc11513h
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C6 H26 As2 F7 N3 O15 V4'
_chemical_formula_weight         866.90
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.894(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8763(6)
_cell_length_b                   14.1659(5)
_cell_length_c                   10.7198(4)
_cell_measurement_reflns_used    46571
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2556.84(16)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans to fill the asymmetric unit'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25614
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.104
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Slab
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0697P)²+42.2332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1845
_reflns_number_gt                3388
_reflns_number_total             4513
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1cc11513h.txt
_cod_data_source_block           2009ek00173mono
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7106416
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N3 N 0.0616(5) 0.4490(7) 0.5692(8) 0.034(2) Uani 1 1 d . . .
H3A H 0.0965 0.4438 0.6386 0.041 Uiso 1 1 calc R . .
H3B H 0.0686 0.3974 0.5191 0.041 Uiso 1 1 calc R . .
N1 N 0.3068(5) 0.3868(6) 0.4535(7) 0.0285(19) Uani 1 1 d . . .
H1A H 0.2643 0.3851 0.3952 0.034 Uiso 1 1 calc R . .
H1B H 0.3508 0.3657 0.4155 0.034 Uiso 1 1 calc R . .
N2 N 0.3737(6) 0.4254(8) 0.6999(9) 0.048(3) Uani 1 1 d . . .
H2A H 0.3302 0.4471 0.7388 0.058 Uiso 1 1 calc R . .
H2B H 0.4168 0.4267 0.7572 0.058 Uiso 1 1 calc R . .
C1 C -0.0207(7) 0.4490(8) 0.6088(10) 0.036(3) Uani 1 1 d . . .
H1C H -0.0265 0.4996 0.6713 0.043 Uiso 1 1 calc R . .
H1D H -0.0317 0.3879 0.6489 0.043 Uiso 1 1 calc R . .
C3 C 0.2911(6) 0.3227(8) 0.5585(9) 0.034(2) Uani 1 1 d . . .
H3C H 0.2840 0.2574 0.5268 0.041 Uiso 1 1 calc R . .
H3D H 0.2416 0.3421 0.5957 0.041 Uiso 1 1 calc R . .
C6 C 0.0794(7) 0.5356(8) 0.5003(11) 0.037(3) Uani 1 1 d . . .
H6A H 0.1335 0.5308 0.4702 0.044 Uiso 1 1 calc R . .
H6B H 0.0785 0.5904 0.5574 0.044 Uiso 1 1 calc R . .
C2 C 0.3588(7) 0.3256(9) 0.6562(10) 0.040(3) Uani 1 1 d . . .
H2C H 0.4072 0.3002 0.6212 0.048 Uiso 1 1 calc R . .
H2D H 0.3463 0.2856 0.7280 0.048 Uiso 1 1 calc R . .
C5 C 0.3205(7) 0.4861(8) 0.4960(12) 0.039(3) Uani 1 1 d . . .
H5A H 0.2721 0.5112 0.5313 0.047 Uiso 1 1 calc R . .
H5B H 0.3328 0.5262 0.4241 0.047 Uiso 1 1 calc R . .
C4 C 0.3887(7) 0.4882(9) 0.5937(11) 0.044(3) Uani 1 1 d . . .
H4A H 0.4379 0.4679 0.5559 0.052 Uiso 1 1 calc R . .
H4B H 0.3968 0.5536 0.6245 0.052 Uiso 1 1 calc R . .
F6 F 0.5775(5) 0.1520(7) 0.6714(9) 0.077(3) Uani 1 1 d . . .
F7 F 0.5240(5) 0.2099(6) 0.4437(11) 0.084(3) Uani 1 1 d . . .
As1 As 0.88269(5) -0.21743(7) 0.19173(8) 0.0195(3) Uani 1 1 d . . .
As2 As 0.65415(6) -0.04515(7) 0.43597(9) 0.0229(3) Uani 1 1 d . . .
V3 V 0.95939(9) -0.16201(11) 0.47270(14) 0.0207(4) Uani 1 1 d . . .
V1 V 0.81289(9) -0.07361(12) 0.62311(14) 0.0219(4) Uani 1 1 d . . .
V4 V 0.82704(10) -0.02011(12) 0.32838(15) 0.0228(4) Uani 1 1 d . . .
V2 V 0.53068(12) 0.10776(14) 0.5376(2) 0.0415(5) Uani 1 1 d . . .
F1 F 0.9440(3) -0.0439(4) 0.3736(5) 0.0285(13) Uani 1 1 d . . .
O4 O 0.7130(4) -0.0483(5) 0.3147(6) 0.0256(15) Uani 1 1 d . . .
O3 O 0.8063(4) -0.0142(5) 0.7510(6) 0.0292(16) Uani 1 1 d . . .
F3 F 0.8343(3) -0.1447(4) 0.4462(5) 0.0209(11) Uani 1 1 d . . .
F5 F 0.5301(3) -0.0273(4) 0.6035(5) 0.0300(13) Uani 1 1 d . . .
F2 F 0.8172(4) 0.0314(5) 0.4990(6) 0.0390(15) Uani 1 1 d . . .
O5 O 0.9327(4) -0.2203(4) 0.0592(5) 0.0196(13) Uani 1 1 d . . .
F4 F 0.9310(4) -0.0899(4) 0.6241(6) 0.0383(15) Uani 1 1 d . . .
O6 O 1.0551(4) -0.1584(5) 0.4932(6) 0.0293(16) Uani 1 1 d . . .
O7 O 0.9494(4) -0.2338(5) 0.3145(6) 0.0240(14) Uani 1 1 d . . .
O8 O 0.8395(4) -0.1090(4) 0.1869(6) 0.0212(14) Uani 1 1 d . . .
O9 O 0.7002(4) -0.0891(5) 0.5677(6) 0.0278(15) Uani 1 1 d . . .
O11 O 0.8086(4) -0.2034(5) 0.6883(6) 0.0228(14) Uani 1 1 d . . .
O10 O 0.8325(4) 0.0772(5) 0.2533(6) 0.0290(16) Uani 1 1 d . . .
O2 O 0.6272(4) 0.0686(5) 0.4569(6) 0.0285(16) Uani 1 1 d . . .
O12 O 0.4238(4) 0.1163(5) 0.6034(6) 0.0284(15) Uani 1 1 d . . .
O1W O 0.4467(5) 0.3608(6) 0.3584(8) 0.0488(12) Uani 1 1 d . . .
O2W O 0.8909(5) 0.2840(6) 0.2710(8) 0.0488(12) Uani 1 1 d . . .
O3W O 0.2527(10) 0.6949(13) 0.8795(16) 0.0488(12) Uani 0.50 1 d P . .
O4W O 0.4411(10) 0.6377(13) 1.3190(16) 0.0488(12) Uani 0.50 1 d P . .
O5W O 0.3055(10) 0.7902(13) 1.0974(16) 0.0488(12) Uani 0.50 1 d P . .
O6W O 0.2960(10) 0.7902(13) 0.6690(16) 0.0488(12) Uani 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 N3 C1 111.8(8) . . ?
C3 N1 C5 112.2(8) . . ?
C4 N2 C2 111.0(8) . . ?
N3 C1 C6 111.1(9) . 3_566 ?
N1 C3 C2 110.3(9) . . ?
N3 C6 C1 111.5(9) . 3_566 ?
C3 C2 N2 110.3(10) . . ?
N1 C5 C4 109.0(10) . . ?
N2 C4 C5 111.1(9) . . ?
O11 As1 O7 112.4(3) 4 . ?
O11 As1 O8 106.6(3) 4 . ?
O7 As1 O8 114.2(3) . . ?
O11 As1 O5 112.2(3) 4 . ?
O7 As1 O5 107.8(3) . . ?
O8 As1 O5 103.4(3) . . ?
O9 As2 O12 107.2(3) . 3_656 ?
O9 As2 O4 111.9(3) . . ?
O12 As2 O4 106.3(3) 3_656 . ?
O9 As2 O2 110.7(3) . . ?
O12 As2 O2 112.9(3) 3_656 . ?
O4 As2 O2 107.7(3) . . ?
O6 V3 O7 99.1(3) . . ?
O6 V3 O5 102.7(3) . 4_556 ?
O7 V3 O5 87.7(3) . 4_556 ?
O6 V3 F1 98.0(3) . . ?
O7 V3 F1 88.5(3) . . ?
O5 V3 F1 159.3(2) 4_556 . ?
O6 V3 F4 99.6(3) . . ?
O7 V3 F4 161.3(3) . . ?
O5 V3 F4 88.6(3) 4_556 . ?
F1 V3 F4 88.5(2) . . ?
O6 V3 F3 171.6(3) . . ?
O7 V3 F3 85.3(2) . . ?
O5 V3 F3 84.5(2) 4_556 . ?
F1 V3 F3 74.9(2) . . ?
F4 V3 F3 76.1(2) . . ?
O3 V1 O9 101.2(3) . . ?
O3 V1 O11 100.3(3) . . ?
O9 V1 O11 86.9(3) . . ?
O3 V1 F2 100.6(3) . . ?
O9 V1 F2 87.7(3) . . ?
O11 V1 F2 159.1(3) . . ?
O3 V1 F4 100.4(3) . . ?
O9 V1 F4 158.3(3) . . ?
O11 V1 F4 87.2(3) . . ?
F2 V1 F4 90.4(3) . . ?
O3 V1 F3 173.3(3) . . ?
O9 V1 F3 84.3(2) . . ?
O11 V1 F3 83.7(2) . . ?
F2 V1 F3 75.6(2) . . ?
F4 V1 F3 74.4(2) . . ?
O10 V4 O4 103.1(3) . . ?
O10 V4 F2 99.1(3) . . ?
O4 V4 F2 90.0(3) . . ?
O10 V4 O8 98.6(3) . . ?
O4 V4 O8 88.2(3) . . ?
F2 V4 O8 162.2(3) . . ?
O10 V4 F1 100.1(3) . . ?
O4 V4 F1 156.6(3) . . ?
F2 V4 F1 88.9(2) . . ?
O8 V4 F1 85.7(2) . . ?
O10 V4 F3 171.8(3) . . ?
O4 V4 F3 83.9(2) . . ?
F2 V4 F3 76.6(2) . . ?
O8 V4 F3 85.7(2) . . ?
F1 V4 F3 73.1(2) . . ?
F6 V2 F7 100.7(5) . . ?
F6 V2 O2 97.1(4) . . ?
F7 V2 O2 90.2(3) . . ?
F6 V2 O12 93.4(3) . . ?
F7 V2 O12 97.4(3) . . ?
O2 V2 O12 165.8(3) . . ?
F6 V2 F5 93.8(4) . . ?
F7 V2 F5 165.1(4) . . ?
O2 V2 F5 84.9(3) . . ?
O12 V2 F5 84.8(3) . . ?
F6 V2 F5 167.7(4) . 3_656 ?
F7 V2 F5 91.5(4) . 3_656 ?
O2 V2 F5 84.8(3) . 3_656 ?
O12 V2 F5 83.0(3) . 3_656 ?
F5 V2 F5 74.2(2) . 3_656 ?
V3 F1 V4 110.9(3) . . ?
As2 O4 V4 124.2(4) . . ?
V3 F3 V4 100.9(2) . . ?
V3 F3 V1 99.1(2) . . ?
V4 F3 V1 97.1(2) . . ?
V2 F5 V2 105.8(2) . 3_656 ?
V4 F2 V1 110.4(3) . . ?
As1 O5 V3 123.6(3) . 4 ?
V3 F4 V1 110.3(3) . . ?
As1 O7 V3 127.7(4) . . ?
As1 O8 V4 127.9(3) . . ?
As2 O9 V1 126.4(4) . . ?
As1 O11 V1 125.9(4) 4_556 . ?
As2 O2 V2 124.2(4) . . ?
As2 O12 V2 125.9(4) 3_656 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N3 C6 1.473(15) . ?
N3 C1 1.478(14) . ?
N1 C3 1.484(13) . ?
N1 C5 1.493(14) . ?
N2 C4 1.480(16) . ?
N2 C2 1.505(16) . ?
C1 C6 1.497(16) 3_566 ?
C3 C2 1.497(14) . ?
C6 C1 1.497(16) 3_566 ?
C5 C4 1.503(17) . ?
F6 V2 1.708(9) . ?
F7 V2 1.762(8) . ?
As1 O11 1.678(6) 4 ?
As1 O7 1.689(6) . ?
As1 O8 1.700(6) . ?
As1 O5 1.702(6) . ?
As2 O9 1.684(6) . ?
As2 O12 1.689(7) 3_656 ?
As2 O4 1.689(6) . ?
As2 O2 1.693(7) . ?
V3 O6 1.616(7) . ?
V3 O7 1.975(7) . ?
V3 O5 1.975(6) 4_556 ?
V3 F1 1.989(6) . ?
V3 F4 2.003(6) . ?
V3 F3 2.125(5) . ?
V1 O3 1.618(7) . ?
V1 O9 1.966(7) . ?
V1 O11 1.970(7) . ?
V1 F2 2.000(6) . ?
V1 F4 2.006(7) . ?
V1 F3 2.199(5) . ?
V4 O10 1.602(7) . ?
V4 O4 1.961(7) . ?
V4 F2 1.987(6) . ?
V4 O8 1.993(6) . ?
V4 F1 2.029(6) . ?
V4 F3 2.169(5) . ?
V2 O2 1.975(7) . ?
V2 O12 1.984(7) . ?
V2 F5 2.039(6) . ?
V2 F5 2.105(6) 3_656 ?
F5 V2 2.105(6) 3_656 ?
O5 V3 1.975(6) 4 ?
O11 As1 1.678(6) 4_556 ?
O12 As2 1.689(7) 3_656 ?
O5W O6W 1.39(2) 4_576 ?
O6W O5W 1.39(2) 4_575 ?
